CN109157454B - Camellia japonica combined extract, preparation method thereof and application thereof in cosmetics - Google Patents
Camellia japonica combined extract, preparation method thereof and application thereof in cosmetics Download PDFInfo
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- CN109157454B CN109157454B CN201811251030.4A CN201811251030A CN109157454B CN 109157454 B CN109157454 B CN 109157454B CN 201811251030 A CN201811251030 A CN 201811251030A CN 109157454 B CN109157454 B CN 109157454B
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
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- A61Q19/08—Anti-ageing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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Abstract
The invention provides a camellia japonica combined extract, a preparation method thereof and an application thereof in cosmetics, wherein the combined extract comprises the following components in percentage by weight: 50-80% of camellia seed supercritical extract, 10-30% of camellia flower leaf supercritical extract and 10-30% of camellia flower leaf residue extract. According to the invention, camellia seed is subjected to supercritical extraction, camellia leaves are mixed and then subjected to supercritical extraction, and camellia leaf residues are further subjected to enzymolysis and alcohol extraction, so that the obtained combined extract contains various active ingredients such as sitosterol, squalene and alpha-VE and high-content oleic acid, and the antioxidant performance is better. The cosmetic prepared from the extract has better effects of moisturizing, locking water, resisting oxidation, improving skin elasticity and the like and repairing skin barriers.
Description
Technical Field
The invention relates to the technical field of deep processing of camellia raw materials, in particular to a camellia combined extract for improving comprehensive utilization of camellia plants, and preparation and application thereof in cosmetics. The camellia japonica combined extract disclosed by the invention has the effects of enhancing the skin oxidation resistance, improving the skin elasticity, improving the skin water locking capacity and the like and repairing skin barriers, and can be used as a functional raw material of high-end cosmetics to be added into the cosmetics.
Background
Camellia (Camellia japonica L.) is a plant of genus Camellia of family Theaceae, belonging to evergreen broadleaf forest tree, also called Camellia, Camellia japonica and winter resistance, and is one of the ten major flowers in China; the camellia has wide distribution and is mainly produced in Zhejiang, Yunnan, Jiangxi, Sichuan and other places in China. The flower, leaf, seed and other parts of the camellia as a natural resource are rich in various bioactive components such as flavone, polyphenol, VE, oleic acid, squalene, phytosterol and other nutrient elements such as calcium, potassium, magnesium, manganese and the like; a large number of researches show that the extract prepared from flowers, leaves and seeds of camellia has good effect of repairing skin barriers, but the effective components of the extract are not fully utilized, and the extract is lack of products with high technological content and high added values.
The supercritical CO2 extraction technology has the advantages of simple process, no organic solvent residue, mild operation conditions, good retention of active ingredients, integration of extraction, concentration and separation and the like, which are incomparable with the traditional process, and is suitable for extracting natural products. But simultaneously, the supercritical extraction technology is suitable for extracting low-molecular, low-polarity, lipophilic and low-boiling-point components, and the extraction rate of active components with strong water solubility and strong polarity is not high; the effective components contained in the camellia, the leaves and the seeds have different properties, and the single supercritical extraction technology cannot meet the comprehensive utilization of plants. The development of comprehensive extraction technology of each active component of the camellia is beneficial to improving the utilization rate of raw materials, reducing the production cost, extracting the active component to the maximum extent and enabling the plant to play the role of the maximum efficiency.
At present, researches on functional components of camellia plants mainly focus on camellia seed oil and a traditional squeezing process, but researches on camellia leaves are relatively few, and particularly, application researches and efficacy test researches on natural extracts developed by taking the camellia leaves as raw materials on skin care products are few; meanwhile, the camellia oil product is mainly an edible product in the market at present and is less applied as a high-end raw material of cosmetics; the existing camellia seed oil refining technology is difficult to refine into high-grade camellia oil special for cosmetics; and the tea oil seeds have strong harvest seasonality, strict storage conditions and easy mildew, rot, oxidation and the like during storage. With the deep research on the efficacy of active ingredients in camellia, camellia leaves and camellia seeds, the development and production of the camellia japonica combined extract with high added value has great potential.
Disclosure of Invention
In order to solve the problem that the existing camellia resources are low in comprehensive utilization degree and fill the blank of camellia raw materials in high-end skin care product raw materials, the invention provides the camellia combined extract, the preparation method thereof and the application thereof in cosmetics.
The purpose of the invention is realized by the following technical scheme:
the invention provides a camellia japonica combined extract which comprises the following components in percentage by weight:
50-80% of supercritical extract of camellia seed,
10-30% of supercritical extract of camellia japonica leaves,
10-30% of the extract of the camellia japonica flower and leaf residue.
Preferably, the camellia japonica combined extract comprises the following components in percentage by weight:
65-75% of supercritical extract of camellia seed,
supercritical extract of leaves of the camellia japonica 15-25%,
10-15% of the camellia japonica flower and leaf residue extract.
Preferably, the raw material variety adopted by the camellia japonica thunbergii with an altitude of more than 500 m is higher than that of the camellia japonica thunbergii in other producing areas, and the content of active ingredients of the obtained extract is higher than that of the camellia japonica thunbergii in other producing areas, especially the content of oleic acid and linoleic acid in camellia seeds.
Preferably, the preparation method of the supercritical extract of the seeds of the camellia japonica comprises the following steps:
a1, pulverizing and sieving camellia seeds, mixing with an anti-coagulating agent, adding activated clay, performing supercritical extraction, and performing two-stage separation;
a2, refining the primary extract obtained in step A1 to obtain the supercritical extract of camellia seeds.
Preferably, in step A1, the step of super-treating is carried outThe parameters for zero-bound extraction were: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-40 ℃; the extraction time is 0.5-1.5 h;
the parameters of the two-stage separation are as follows: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the II-grade separation pressure is 5-6Mpa, and the temperature is 25-40 ℃; more preferably, the separation temperature for stage II is from 25 to 30 ℃.
The addition amount of the anti-coagulating agent is 5-10% of the weight of the camellia seed, and the addition amount of the activated clay is 2-10% of the weight of the camellia seed.
Preferably, the active ingredients of the supercritical extract of the seeds of the camellia japonica have squalene content of 250-350ppm, vitamin E content of 150-250ppm and beta-sitosterol content of 80-120 ppm.
Preferably, the crushing mesh of the camellia seeds is 80 meshes, and the sieving rate of particles is more than or equal to 98%.
Preferably, the anti-agglomerating agent is silica.
In the preparation method of the supercritical extract of the camellia seed, the active clay is added to decolor the extracted camellia seed oil; the two-stage separation can separate phospholipid substances and wax substances from the camellia seed oil to replace degumming and winterization treatment of the camellia seed oil; the refining treatment comprises the steps of deacidification, dehydration and deodorization.
Preferably, the preparation method of the supercritical extract of the camellia japonica leaves comprises the following steps:
b1, mixing the camellia japonica flower and the camellia japonica leaf, crushing, sieving, performing supercritical extraction, and performing two-stage separation;
b2, refining and filtering the primary extract obtained in the step B1 to obtain the supercritical extract of the seeds of the camellia and the flower and leaf residue of the camellia.
Preferably, in step B1, the camellia japonica leaves comprise camellia japonica flowers and camellia japonica leaves in a mass ratio of 1:1-4, more preferably in a ratio of 1: 2;
the parameters of the supercritical extraction are as follows: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-50 ℃; the extraction time is 1-2 h;
the parameters of the two-stage separation are as follows: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the II-grade separation pressure is 7-8Mpa, and the temperature is 25-40 ℃;
in step B2, the filtration is performed with a 0.1-0.22um filter membrane.
Preferably, the crushing mesh number of the camellia japonica flower and the camellia japonica leaf is 80 meshes, and the sieving rate of particles is more than or equal to 98%.
Preferably, the preparation method of the camellia japonica flower and leaf residue extract comprises the following steps:
c1, adding enzyme preparation and alcohol solvent into the camellia leaves residue obtained by the method of claim 6, stirring and reacting to obtain camellia leaves residue enzymatic hydrolysis alcohol extract;
c2, carrying out rough filtration on the camellia japonica leaf residue enzymatic hydrolysis alcohol extract, and carrying out vacuum concentration on the obtained filtrate to obtain an extract;
and C2, re-dissolving the extract, and refining to obtain the camellia japonica residue extract.
Preferably, in step C1, the enzyme preparation comprises: pectinase 0.1-0.5 ‰ of the weight of the flos Camelliae Japonicae residue, cellulase 1-5 ‰ of the weight of the flos Camelliae Japonicae residue, and amylase 1-5 ‰ of the weight of the flos Camelliae Japonicae residue; the adding amount of the solvent is 15-20 times of the weight of the camellia japonica flower and leaf residue; the conditions of the stirring reaction are as follows: the reaction temperature is 40-50 ℃, the reaction time is 30-60min, and the stirring speed is 100-;
in the step C2, the vacuum concentration temperature is 50-55 ℃, and the vacuum concentration is carried out until the volume of the filtrate is 1/12-1/16, and the selection of the concentration multiple is proved by previous experiments to be more beneficial to improving the stability of the extract in the cosmetic camellia japonica composition extract system;
in the step C3, the components adopted for re-dissolving are absolute ethyl alcohol and hydrogenated castor oil, the hydrogenated castor oil is easily dissolved in the ethyl alcohol, and the ethyl alcohol can furthest reserve hydrophilic active ingredients such as flavone, polyphenol and the like in the camellia; in the solution obtained by redissolution, the mass percentage of each component is as follows: 1-5% of extract, 40-50% of absolute ethyl alcohol and 40-50% of hydrogenated castor oil; the refining treatment comprises ceramic membrane filtration and ultrafiltration membrane filtration.
More preferably, in the step C1, the alcohol solvent is 60-80% ethanol solution by mass fraction, and more preferably 70% ethanol solution;
in step C2, the concentration is to 1/12 of the filtrate volume;
in the step C3, the aperture of the ceramic membrane is 30-200nm, and the cut-off molecular weight of the ultrafiltration membrane is 2000Da-5000 Da.
According to the invention, camellia seed is subjected to supercritical extraction, camellia leaves are mixed and then subjected to supercritical extraction, and camellia leaf residues are further subjected to enzymolysis and alcohol extraction, so that the obtained combined extract contains various active ingredients such as sitosterol, squalene and alpha-VE and high-content oleic acid, and the antioxidant performance is better.
The invention also provides a preparation method of the camellia japonica combined extract, which comprises the step of mixing the components in proportion.
The invention also provides application of the camellia japonica combined extract in cosmetics, and particularly relates to application of the camellia japonica combined extract in cosmetic products such as skin moistening oil, emulsion, cream and the like with skin barrier repairing effects, such as skin elasticity improvement, moisture preservation, water locking, oxidation resistance and the like.
Compared with the prior art, the invention has the following beneficial effects:
1. the camellia combined extract contains 3 parts of flowers, leaves and seeds of the camellia, and the raw materials are comprehensively utilized; meanwhile, the screened raw material variety is Zhejiang red camellia variety with the altitude of more than 500 m, and compared with camellia in other producing areas and other varieties, the content of active ingredients is higher, especially the content of oleic acid and linoleic acid in camellia seeds.
2. The camellia seeds are subjected to supercritical extraction, so that active ingredients are effectively reserved, and the pollution of solvent use to the environment is avoided; the method has the more prominent characteristics that the decoloring and degumming procedures of the camellia seeds are avoided through the process improvement in the supercritical extraction, the post-treatment refining link is reduced, and the method is more environment-friendly and energy-saving.
3. After the effective components of the camellia and the camellia leaves are extracted by supercritical extraction and enzymolysis alcohol extraction, fat-soluble weak-polarity active substances and alcohol-soluble strong-polarity active substances are extracted to the maximum extent; through the chemical properties of absolute ethyl alcohol and castor oil, the fat-soluble weak polar active substance and the alcohol-soluble strong polar active substance are scientifically compounded, compatible and coexistent, and the system is balanced.
4. After the camellia leaves are subjected to supercritical high-pressure treatment (15-30Mpa), the cell disruption degree is higher, and the dissolution of active substances is synergistically promoted, so that the active ingredients in camellia leaf residues are more fully extracted.
5. By enzymolysis, the indissolvable components in the camellia leaves can be promoted to be effectively converted into soluble components, further damage of a tissue structure is promoted along with the deepening of enzyme reaction, the permeability of cell walls and cell membranes is increased, the release and leaching of endogenous substances are facilitated, and the deep proceeding of the reaction is facilitated; the tissue structure of camellia leaves becomes loose under the action of the enzyme, the camellia leaves are separated from liquid in the pulp, the subsequent processing process is improved, the time of the separation, filtration and other operation processes is shortened, and the process realizability is high.
6. According to the invention, the camellia japonica seeds are subjected to supercritical extraction, the camellia japonica leaves are mixed and then subjected to supercritical extraction, and the camellia japonica leaf residues are further subjected to enzymolysis and alcohol extraction, so that the obtained combined extract is rich in various active ingredients such as sitosterol, squalene, α -VE and the like and high-content oleic acid, has better oxidation resistance, better skin elasticity improving effect and obvious effect of reducing percutaneous water loss, and test results show that the DPPH clearance rate can be up to 89%, the change rate of the skin elasticity R2 value can be up to 8.32%, and the percutaneous water loss rate after 4 weeks can be as low as 21.14 g/(h.m)2)。
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides a preparation method of a camellia japonica combined extract, which comprises the following steps:
1. selecting red flower tea-oil tree of Zhejiang Lishui Da Yang as raw material, and selecting camellia seed, camellia flower and camellia leaf.
2. Preparing a supercritical extract of camellia seeds:
2.1, crushing and sieving the camellia seeds, wherein the crushing mesh number is 80 meshes, and the sieving rate of particles is more than or equal to 98 percent;
2.2 adding 5 wt% of silica as anti-coagulant into the sieved camellia seeds, stirring, placing into an extraction kettle, and placing activated clay into the extraction kettle, wherein the addition amount of the activated clay is 5 wt% of the camellia seeds, the activated clay is arranged at the upper part of the extraction kettle, and supercritical CO is adopted2And entering from the bottom of the extraction kettle through a high-pressure pump. The activated clay is laid on the upper layer, which is beneficial to the decolorization of camellia seed oil in the process of camellia seed extraction.
2.3 setting the parameters of the supercritical extraction: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-40 ℃; the extraction time is 0.5-1.5 h; performing supercritical extraction, and performing two-stage separation at a pressure of 8-12Mpa and a temperature of 25 deg.C; the separation pressure of stage II is 5-6Mpa, and the temperature is 30 deg.C.
2.4 refining the primary extract obtained after the treatment of the step 2.3, specifically deacidifying, dehydrating and deodorizing to obtain the supercritical extract of the seeds of the camellia, wherein the content of active ingredients is as follows: the squalene content is 350ppm, the vitamin E content is 250ppm, and the beta-sitosterol content is 120 ppm.
3. Preparation of supercritical extract of camellia japonica leaves
3.1 mixing the camellia japonica flower and the camellia japonica leaf according to the proportion of 1:2, crushing and sieving, wherein the crushing mesh number is 80 meshes, and the sample sieving rate is more than or equal to 98%.
3.2 carrying out supercritical extraction on the screened camellia seeds, and then carrying out two-stage separation; parameters of supercritical extraction: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-50 ℃; the extraction time is 1-2 h; two stage separationThe parameters of (A) are as follows: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the separation pressure of stage II is 7-8Mpa, and the temperature is 25-40 deg.C.
3.3 refining and filtering the primary extract obtained in the step 3.2, and filtering the primary extract by a filter membrane of 0.1-0.22um to obtain the supercritical extract of the seeds of the camellia and the residue of the leaves of the camellia.
4. Preparation method of camellia japonica flower and leaf residue extract
4.1 adding pectinase accounting for 0.1 per thousand of the weight of the camellia leaves residues, cellulase accounting for 5 per thousand of the weight of the camellia leaves residues and amylase accounting for 2.5 per thousand of the weight of the camellia leaves residues into the camellia leaves residues obtained in the step 3.3 to serve as an enzyme preparation, adding an ethanol solution accounting for 20 times of the weight of the camellia leaves residues (the mass fraction is 70%), stirring and reacting at 40-50 ℃ for 30-60min at the stirring speed of 100rpm/min to obtain the camellia leaves residues enzymatic hydrolysis alcohol extract.
4.2 after the camellia japonica leaves residue is subjected to enzymolysis and alcohol extraction rough filtration, the obtained filtrate is concentrated in vacuum; the vacuum concentration condition is that the heating temperature of a rotary evaporator is 50-55 ℃; concentrating to 1/12 of the filtrate to obtain extract.
4.3 dissolving the extract with anhydrous ethanol and hydrogenated castor oil to obtain a re-dissolved substance, wherein the extract accounts for 1-5%; the proportion of the absolute ethyl alcohol is 40-50%, and the proportion of the hydrogenated castor oil is 40-50%.
4.4 refining the re-dissolved substance by integrated membrane separation technology, specifically comprising filtering with ceramic membrane with aperture of 30nm and ultrafiltration membrane with cut-off molecular weight of 2000Da to obtain the camellia japonica residue extract.
5. And mixing the prepared camellia seed supercritical extract, the camellia flower and leaf supercritical extract and the camellia flower and leaf residue extract according to the mass ratio of 70%, 20% and 10% to prepare the camellia combined extract.
Example 2
The embodiment provides a preparation method of a camellia japonica combined extract, which comprises the following steps:
1. selecting red flower tea-oil tree of Zhejiang Lishui Da Yang as raw material, and selecting camellia seed, camellia flower and camellia leaf.
2. Preparing a supercritical extract of camellia seeds:
2.1, crushing and sieving the camellia seeds, wherein the crushing mesh number is 80 meshes, and the sieving rate of particles is more than or equal to 98 percent;
2.2 adding anti-coagulant silicon dioxide 10% of the weight of the camellia seed into the screened camellia seed, uniformly stirring, putting into an extraction kettle, and putting activated clay into the extraction kettle, wherein the addition amount of the activated clay is 10% of the weight of the camellia seed, the activated clay is arranged at the upper part of the extraction kettle, and supercritical CO is adopted2And entering from the bottom of the extraction kettle through a high-pressure pump. The activated clay is laid on the upper layer, which is beneficial to the decolorization of camellia seed oil in the process of camellia seed extraction.
2.3 setting the parameters of the supercritical extraction: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-40 ℃; the extraction time is 0.5-1.5 h; performing supercritical extraction, and performing two-stage separation at a pressure of 8-12Mpa and a temperature of 40 deg.C; the separation pressure of II-stage is 5-6Mpa, and the temperature is 40 deg.C.
2.4 refining the primary extract obtained after the treatment of the step 2.3, specifically deacidifying, dehydrating and deodorizing to obtain the supercritical extract of the seeds of the camellia, wherein the content of active ingredients is as follows: the content of squalene is 300ppm, the content of vitamin E is 150ppm, and the content of beta-sitosterol is 100 ppm.
3. Preparation of supercritical extract of camellia japonica leaves
3.1 mixing the camellia japonica flower and the camellia japonica leaf according to the proportion of 1:1, crushing and sieving, wherein the crushing mesh number is 80 meshes, and the sample sieving rate is more than or equal to 98%.
3.2 carrying out supercritical extraction on the screened camellia seeds, and then carrying out two-stage separation; parameters of supercritical extraction: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-50 ℃; the extraction time is 1-2 h; the parameters for the two-stage separation are: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the separation pressure of stage II is 7-8Mpa, and the temperature is 25-40 deg.C.
3.3 refining and filtering the primary extract obtained in the step 3.2, and filtering the primary extract by a filter membrane of 0.1-0.22um to obtain the supercritical extract of the seeds of the camellia and the residue of the leaves of the camellia.
4. Preparation method of camellia japonica flower and leaf residue extract
4.1 adding pectinase accounting for 0.5 per thousand of the weight of the camellia leaf residues, cellulase accounting for 1 per thousand of the weight of the camellia leaf residues and amylase accounting for 5 per thousand of the weight of the camellia leaf residues into the camellia leaf residues obtained in the step 3.3 to serve as enzyme preparations, adding an ethanol solution (with the mass fraction of 60%) accounting for 15 times of the weight of the camellia leaf residues, stirring and reacting at 40-50 ℃ for 30-60min at the stirring speed of 100-200rpm/min to obtain the camellia leaf residue enzymatic hydrolysis alcohol extract.
4.2 after the camellia japonica leaves residue is subjected to enzymolysis and alcohol extraction rough filtration, the obtained filtrate is concentrated in vacuum; the vacuum concentration condition is that the heating temperature of a rotary evaporator is 50-55 ℃; concentrating to 1/16 of the filtrate to obtain extract.
4.3 dissolving the extract by using absolute ethyl alcohol and castor oil, wherein the extract accounts for 1-5 percent; the proportion of the absolute ethyl alcohol is 40-50%, and the proportion of the hydrogenated castor oil is 40-50%, so as to obtain a re-dissolved substance.
4.4 refining the re-dissolved substance by integrated membrane separation technology, specifically comprising filtering with ceramic membrane with aperture of 100nm and ultrafiltration membrane with molecular weight cutoff of 5000Da to obtain the camellia flower and leaf residue extract.
5. Mixing the prepared camellia seed supercritical extract, the camellia flower and leaf supercritical extract and the camellia flower and leaf residue extract according to the mass ratio of 60%, 30% and 10% to prepare the camellia combined extract.
Example 3
The embodiment provides a preparation method of a camellia japonica combined extract, which comprises the following steps:
1. selecting red flower tea-oil tree of Zhejiang Lishui Da Yang as raw material, and selecting camellia seed, camellia flower and camellia leaf.
2. Preparing a supercritical extract of camellia seeds:
2.1, crushing and sieving the camellia seeds, wherein the crushing mesh number is 80 meshes, and the sieving rate of particles is more than or equal to 98 percent;
2.2 mixing the sieved camellia seeds with anti-coagulant silicon dioxide which accounts for 8 percent of the weight of the camellia seeds, uniformly stirring and placing the mixture into an extraction kettle, and then placing activated clay into the extraction kettle for extractionAdding activated clay 2 wt% of camellia seeds in the kettle, wherein the activated clay is arranged at the upper part of the extraction kettle, and supercritical CO is added2And entering from the bottom of the extraction kettle through a high-pressure pump. The activated clay is laid on the upper layer, which is beneficial to the decolorization of camellia seed oil in the process of camellia seed extraction.
2.3 setting the parameters of the supercritical extraction: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-40 ℃; the extraction time is 0.5-1.5 h; performing supercritical extraction, and performing two-stage separation at a pressure of 8-12Mpa and a temperature of 25 deg.C; the separation pressure of II-stage is 5-6Mpa, and the temperature is 25 deg.C.
2.4 refining the primary extract obtained after the treatment of the step 2.3, specifically deacidifying, dehydrating and deodorizing to obtain the supercritical extract of the seeds of the camellia, wherein the content of active ingredients is as follows: the content of squalene is 250ppm, the content of vitamin E is 200ppm, and the content of beta-sitosterol is 80 ppm.
3. Preparation of supercritical extract of camellia japonica leaves
3.1 mixing the camellia japonica flower and the camellia japonica leaf according to the proportion of 1:4, crushing and sieving, wherein the crushing mesh number is 80 meshes, and the sample sieving rate is more than or equal to 98%.
3.2 carrying out supercritical extraction on the screened camellia seeds, and then carrying out two-stage separation; parameters of supercritical extraction: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-50 ℃; the extraction time is 1-2 h; the parameters for the two-stage separation are: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the separation pressure of stage II is 7-8Mpa, and the temperature is 25-40 deg.C.
3.3 refining and filtering the primary extract obtained in the step 3.2, and filtering the primary extract by a filter membrane of 0.1-0.22um to obtain the supercritical extract of the seeds of the camellia and the residue of the leaves of the camellia.
4. Preparation method of camellia japonica flower and leaf residue extract
4.1 adding pectinase accounting for 0.3 per thousand of the weight of the camellia leaves residues, cellulase accounting for 2 per thousand of the weight of the camellia leaves residues and amylase accounting for 1 per thousand of the weight of the camellia leaves residues into the camellia leaves residues obtained in the step 3.3 to serve as an enzyme preparation, adding an ethanol solution accounting for 20 times of the weight of the camellia leaves residues (the mass fraction is 80 percent), stirring and reacting at 40-50 ℃ for 30-60min at the stirring speed of 100-200rpm/min to obtain the camellia leaves residues enzymatic hydrolysis alcohol extract.
4.2 after the camellia japonica leaves residue is subjected to enzymolysis and alcohol extraction rough filtration, the obtained filtrate is concentrated in vacuum; the vacuum concentration condition is that the heating temperature of a rotary evaporator is 50-55 ℃; concentrating to 1/15 of the filtrate to obtain extract.
4.3 dissolving the extract by using absolute ethyl alcohol and castor oil, wherein the extract accounts for 1-5 percent; the proportion of the absolute ethyl alcohol is 40-50%, and the proportion of the hydrogenated castor oil is 40-50%, so as to obtain a re-dissolved substance.
4.4 refining the re-dissolved substance by integrated membrane separation technology, specifically comprising filtering with ceramic membrane with pore diameter of 200nm and ultrafiltration membrane with molecular weight cutoff of 3000Da to obtain the camellia flower and leaf residue extract.
5. And mixing the prepared camellia seed supercritical extract, the camellia flower and leaf supercritical extract and the camellia flower and leaf residue extract according to the mass ratio of 80%, 10% and 10% to prepare the camellia combined extract.
Example 4
This example provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 3, except that: the camellia seed supercritical extract, the camellia flower leaf supercritical extract and the camellia flower leaf residue extract are mixed according to the mass ratio of 50%, 20% and 30% to prepare the camellia combined extract.
Example 5
This example provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: and mixing 65%, 25% and 10% of camellia japonica seed supercritical extract, camellia japonica leaf supercritical extract and camellia japonica leaf residue extract according to the mass ratio to obtain the camellia japonica combined extract.
Example 6
This example provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: and mixing the camellia seed supercritical extract, the camellia flower leaf supercritical extract and the camellia flower leaf residue extract according to the mass ratio of 75%, 15% and 10% to obtain the camellia combined extract.
Example 7
This example provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: and mixing the camellia seed supercritical extract, the camellia flower leaf supercritical extract and the camellia flower leaf residue extract according to the mass ratio of 70%, 15% and 15% to obtain the camellia combined extract.
Comparative example of example 1:
comparative examples 1 to 1
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: no anti-coagulant was added in step 2.2 of this comparative example. During extraction, camellia seed materials are seriously agglomerated and are insufficiently extracted, and the obtained supercritical camellia seed extract has the following active component contents: the squalene content is 150ppm, the vitamin E content is 100ppm, and the beta-sitosterol content is 80 ppm.
Comparative examples 1 to 2
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: no activated clay was added in step 2.2 of this comparative example. The supercritical extract material of the camellia seed oil after extraction has darker color, and the refining treatment process is increased, so that the content of active ingredients of the supercritical extract of the camellia seed is as follows: the squalene content is 100ppm, the vitamin E content is 150ppm, and the beta-sitosterol content is 100 ppm.
Comparative examples 1 to 3
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: this comparative example did not undergo the treatment of step 4, and the method of step 5 was: and mixing the prepared camellia seed supercritical extract and the camellia flower leaf supercritical extract according to the mass ratio of 70% and 30% to obtain the camellia combined extract.
Comparative examples 1 to 4
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: the method of step 5 in this comparative example is: mixing the prepared camellia seed supercritical extract, the camellia flower and leaf supercritical extract and the camellia flower and leaf residue extract according to the mass ratio of 50%, 30% and 20% to prepare the camellia combined extract.
Comparative examples 1 to 5
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: step 2 of this comparative example is to prepare the camellia seed extract by conventional pressing, filtering and decoloring.
Comparative examples 1 to 6
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 1, except that: step 3 of this comparative example is to prepare the camellia flower and leaf extract and camellia flower and leaf residue by percolation extraction at room temperature.
Comparative example of example 2:
comparative example 2-1
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 2, except that: in step 2.3 of this comparative example, only a stage I separation was performed, and no stage II separation was performed. Insufficient separation after extraction, which results in high content of impurity components in the obtained camellia seed supercritical extract, and the content of active ingredients in the obtained camellia seed supercritical extract is as follows: the squalene content is 150ppm, the vitamin E content is 100ppm, and the beta-sitosterol content is 80 ppm.
Comparative examples 2 to 2
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 2, except that: in step 2.3 of this comparative example, an extraction pressure of 10MPa was used. The supercritical extract of the obtained camellia seeds comprises the following active components: the squalene content is 180ppm, the vitamin E content is 120ppm, and the beta-sitosterol content is 90 ppm.
Comparative examples 2 to 3
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 2, except that: in step 3.1 of the comparative example, the mixing ratio of the camellia japonica flower to the camellia japonica leaf is 2: 1.
Comparative examples 2 to 4
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 2, except that: in step 3 of the comparative example, the camellia leaves are not contained, and the obtained product is a supercritical extract of camellia japonica; the product obtained in the step 4 is the camellia japonica residue extract.
Comparative example of example 3:
comparative example 3-1
This comparison provides a method for preparing a camellia japonica thunb combined extract, which is substantially the same as the method of example 3, except that: in the comparative example, the step of supercritical extraction of the camellia leaves is not carried out, and the step 4.1 does not adopt camellia leaf residues for extraction preparation, but directly adopts the raw materials in the step 3.1 to carry out the enzymolysis and alcohol extraction in the step 4, so as to obtain the camellia leaf enzymolysis and alcohol extraction product.
Comparative examples 3 to 2
The comparative example provides a preparation method of a camellia japonica combined extract, which comprises the following steps:
1. same as in step 1 of example 3.
2. Preparing a supercritical extract of camellia seeds: same as in step 2 of example 3.
3. Preparing a supercritical extract of the camellia japonica: prepared using the method of steps 3 and 4 in example 3.
4. Preparing a supercritical extract of the camellia japonica leaves: prepared using the method of steps 3 and 4 in example 3.
5. Mixing the camellia seed supercritical extract, the camellia flower supercritical extract and the camellia leaf supercritical extract according to the mass ratio of 80%, 10% and 10% to obtain the camellia combined extract.
Effect verification experiment 1：
The camellia japonica thunb combined extract prepared in all the examples and comparative examples is subjected to an antioxidant test of DPPH free radical scavenging rate, and meanwhile, in order to observe the antioxidant capacity of the camellia japonica thunb combined extract more intuitively, a common antioxidant Vc is selected as a control. The specific method comprises the following steps:
the experimental steps are as follows: adding 2mL of DPPH ethanol solution and 2mL of sample to be detected (Camellia japonica Linne combined extract, Vc) solution into the test tube, shaking, mixing uniformly, reacting in dark for 30min, measuring light absorption value A at 517nm, and measuring light absorption value A of mixed solution of 2mL of DPPH ethanol solution and 2mL of anhydrous ethanol0And the light absorption value A of the mixed solution of 2mL of absolute ethyl alcohol and 2mL of sample to be detectedbCalculate DPPH-free radical clearance:
DPPH.radical scavenging ratio (%) - (A)0-(A-Ab))/A0×100
The results of the tests are shown in table 1, the higher the DPPH clearance of the extract, the stronger the antioxidant properties of the extract. The result shows that the comparative example is obviously different from the example 1, and simultaneously the antioxidant capacity of the camellia japonica combined extract is better than that of the VC solution.
TABLE 1
| Numbering | DPPH clearance (%) | Numbering | DPPH clearance (%) |
| Vc solution (control group) | 70 | Comparative examples 1 to 3 | 81 |
| Example 1 | 89 | Comparative examples 1 to 4 | 74 |
| Example 2 | 85 | Comparative examples 1 to 5 | 72 |
| Example 3 | 83 | Comparative examples 1 to 6 | 79 |
| Example 4 | 83 | Comparative example 2-1 | 83 |
| Example 5 | 87 | Comparative examples 2 to 2 | 82 |
| Example 6 | 86 | Comparative examples 2 to 3 | 76 |
| Example 7 | 87 | Comparative examples 2 to 4 | 73 |
| Comparative examples 1 to 1 | 80 | Comparative example 3-1 | 78 |
| Comparative examples 1 to 2 | 78 | Comparative examples 3 to 2 | 75 |
Effect verification experiment 2:
the camellia japonica thunb combined extract prepared in all the examples and the comparative examples is subjected to a human body safety patch test, and the test method refers to a human body skin patch test in 2015 cosmetic safety technical specification. The method for the skin closed patch test comprises the following steps: selecting 30 persons with age of 18-60 years, selecting the persons with area not more than 50mm2And qualified spot test equipment with the depth of about 1mm, 0.020mL of the camellia sinensis combined extract prepared in the above examples and comparative examples is put into a small chamber of the spot test equipment, a control hole is a blank control (no substance is put), the spot test equipment added with the camellia sinensis combined extract is pasted on the curved side of the forearm of a subject by using a hypoallergenic adhesive tape, and the speckle test equipment is lightly pressed by hands and uniformly pasted on the skin for 24 hours. Observing skin reactions according to the standard of the table 2 after 30min (after the indentation disappears), 24h and 48h after the test device containing the red camellia combined extract is removed, and recording the observation results. The patch test results of the camellia japonica combined extract are shown in table 3.
The experimental results show that the camellia japonica thunb combined extract prepared in all the examples and the comparative examples passes the human body patch safety test.
TABLE 2 skin response grading Standard for skin Enclosed Patch test
TABLE 3 human body safety test results
Effect verification experiment 3:
the combined extract of camellia japonica prepared in all the above examples and comparative examples is diluted with a certain solvent and then subjected to a human skin elasticity test, wherein the test apparatus is a skin elasticity tester (Cutometer dual MPA580), and the test method is as follows: 30 healthy women are selected for each group of camellia japonica combined extract diluted samples, the age is 30 +/-2 years old, the samples are smeared on the cheeks, the skin elasticity test is carried out on the samples before smearing and after the samples are used for four weeks by using an instrument, the skin elasticity test is carried out for 3 times in parallel, the average value is taken, and the R2 value is recorded.
Wherein each group of the camellia japonica combined extract samples are diluted by olive oil, and the preparation proportion is that the camellia japonica combined extract: olive oil 1: 9.
Wherein, the change rate is relative to the change rate before use, and the calculation formula is as follows:
delta after four weeks is T4-T0
In the formula, T0-pre-cosmetic R2 value for the test area.
T4R2 value after four weeks of application of the cosmetic to the test area.
N-number of subjects.
Meanwhile, in order to more visually observe the effect of the camellia japonica combined extract on improving the skin elasticity and deduct the influence of the olive oil on the skin elasticity, the olive oil is used as a blank control.
The test results are shown in Table 4, where the closer the R2 value to 1, the better the skin elasticity. The higher the rate of change of the R2 value, the better the effect of the sample in increasing skin elasticity. The comparative example is obviously different from the example 1, and meanwhile, the camellia japonica combined extract has a better effect of improving the skin elasticity.
TABLE 4
Effect verification experiment 4:
the combined extract of camellia japonica prepared in all the above examples and comparative examples was diluted with a solvent and tested for human transdermal water loss by a skin surface water loss tester Tewameter TM 300 (CK, germany) according to the following test methods: 30 healthy women are selected for each group of camellia japonica combined extract diluted samples, the age is 30 +/-2 years old, the samples are smeared on the cheeks, the percutaneous water loss measurement is carried out on the samples before smearing and after the samples are used for four weeks by using an instrument, the samples are tested in parallel for 3 times, the average value is taken, and the percutaneous water loss value is recorded.
Wherein each group of the camellia japonica combined extract samples are diluted by olive oil, and the preparation proportion is that the camellia japonica combined extract: olive oil 1: 9.
Wherein, the change rate is relative to the change rate before use, and the calculation formula is as follows:
delta after four weeks is A4-A0
In the formula, A0-transdermal water loss value before application of cosmetic to the test area.
A4-value of transdermal water loss after four weeks of application of the cosmetic to the test area.
N-number of subjects.
Meanwhile, in order to more intuitively observe the effect of the camellia japonica combined extract on improving the skin water-locking capacity and deduct the influence of olive oil on the skin water-locking capacity, the olive oil is used as a blank control.
The smaller the value of the percutaneous water loss rate is, the less the water loss is, the stronger the water-locking capacity is, and the better the barrier of the skin is.
The statistical results of the percutaneous water loss rate are shown in Table 5. The results show that: all examples and comparative examples showed a significant reduction in the value of the trans-dermal water loss after application, and in particular example 1 showed a significant reduction in trans-dermal water loss, i.e. a significant skin barrier repair effect.
TABLE 5
Application example 1
This example provides an emollient oil comprising the following formulation components: the camellia japonica thunb oil composition comprises 10% of camellia japonica thunb combined extract, 20% of wheat germ oil, 20% of sweet almond oil, 20% of common selfheal fruit oil, 10% of macadamia nut oil, 5% of jojoba seed oil, 5% of brickey fruit oil, 5% of aloe oil, 5% of rose hip oil, 0.5% of plant alkane, 0.2% of tocopherol acetate, 0.2% of phytosterol, 0.02% of carnosic acid and 0.2% of plant squalane.
The preparation method of the skin moisturizing oil comprises the following steps:
1) adding the above composition into an emulsifying pot at 85 + -5 deg.C, and keeping the temperature for 60min until the mixture is clear and transparent;
2) cooling to below 50 deg.C, adding the selected essence, stirring and mixing uniformly (speed 50 r/min);
3) filtering with 10um end filter to obtain skin caring oil containing herba Camelliae Japonicae extract.
The stability of the obtained emollient oil is inspected, the safety of the emollient oil is inspected, the compatibility of packaging materials is tested, and the human body efficacy is tested, and the results show that the camellia emollient oil used in the research has no chemical preservative and has zero burden on the skin; meanwhile, the added camellia combined extract contains a plurality of active ingredients such as sitosterol, squalene, alpha-VE and the like and high-content oleic acid, so that the camellia combined extract has the effects of better skin affinity, oxidation resistance, aging resistance, inflammation resistance, bacteria resistance, skin barrier protection and the like on the skin; the camellia soothing oil has better repairing effects of moisturizing, locking water, increasing skin elasticity, lubricating skin and resisting oxidation by combining other components in the camellia soothing oil.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (5)
1. The camellia japonica combined extract is characterized by comprising the following components in percentage by weight:
65-75% of supercritical extract of camellia seed,
supercritical extract of leaves of the camellia japonica 15-25%,
10-15% of camellia japonica flower and leaf residue extract;
the preparation method of the supercritical extract of the camellia seeds comprises the following steps:
a1, pulverizing and sieving camellia seeds, mixing with an anti-coagulating agent, adding activated clay, performing supercritical extraction, and performing two-stage separation;
a2, refining the primary extract obtained in step A1 to obtain the supercritical extract of camellia seeds;
in the step A1, the extraction pressure of the supercritical extraction is 15-30 Mpa;
the preparation method of the supercritical extract of the camellia japonica leaves comprises the following steps:
b1, mixing the camellia japonica flower and the camellia japonica leaf, crushing, sieving, performing supercritical extraction, and performing two-stage separation;
b2, refining and filtering the primary extract obtained in the step B1 to obtain a supercritical extract of the leaves of the camellia japonica and residues of the leaves of the camellia japonica;
in the step B1, the camellia japonica leaves comprise camellia japonica flowers and camellia japonica leaves in a mass ratio of 1: 1-4;
the preparation method of the camellia japonica flower and leaf residue extract comprises the following steps:
c1, adding an enzyme preparation and an alcohol solvent into the camellia leaves residue obtained by the method of the step B2, and stirring for reaction to obtain a camellia leaves residue enzymatic hydrolysis alcohol extract;
c2, carrying out rough filtration on the camellia japonica leaf residue enzymatic hydrolysis alcohol extract, and carrying out vacuum concentration on the obtained filtrate to obtain an extract;
c2, re-dissolving the extract, and refining to obtain the camellia japonica residue extract;
in step C1, the enzyme preparation comprises: pectinase 0.1-0.5 ‰ of the weight of the flos Camelliae Japonicae residue, cellulase 1-5 ‰ of the weight of the flos Camelliae Japonicae residue, and amylase 1-5 ‰ of the weight of the flos Camelliae Japonicae residue; the adding amount of the solvent is 15-20 times of the weight of the camellia japonica flower and leaf residue; the conditions of the stirring reaction are as follows: the reaction temperature is 40-50 ℃, the reaction time is 30-60min, and the stirring speed is 100-;
in step C2, the temperature of vacuum concentration is 50-55 ℃, and the concentration is carried out until the filtrate volume is 1/12-1/16;
in the step C3, the components adopted for re-dissolving are absolute ethyl alcohol and hydrogenated castor oil; in the solution obtained by redissolution, the mass percentage of each component is as follows: 1-5% of extract, 50-70% of absolute ethyl alcohol and 50-70% of hydrogenated castor oil; the refining treatment comprises ceramic membrane filtration and ultrafiltration membrane filtration.
2. The camellia reticulata combination extract of claim 1, wherein in step a1, the supercritical extraction parameters are: CO22The flow rate of the fluid is 15-30 ml/min; the extraction temperature is 30-40 ℃; the extraction time is 0.5-1.5 h;
the parameters of the two-stage separation are as follows: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the II-grade separation pressure is 5-6Mpa, and the temperature is 25-40 ℃;
the addition amount of the anti-coagulating agent is 5-10% of the weight of the camellia seed, and the addition amount of the activated clay is 2-10% of the weight of the camellia seed.
3. The camellia japonica thunb combination extract as claimed in claim 1, wherein the active ingredients of the supercritical extract of camellia japonica thunb seeds comprise squalene content of 250-350ppm, vitamin E content of 150-250ppm and beta-sitosterol content of 80-120 ppm.
4. The camellia reticulata combination extract of claim 1, wherein in step B1, the supercritical extraction parameters are: CO22The flow rate of the fluid is 15-30 ml/min; the extraction pressure is 15-30 Mpa; the extraction temperature is 30-50 ℃; the extraction time is 1-2 h;
the parameters of the two-stage separation are as follows: the separation pressure of the I grade is 8-12Mpa, and the temperature is 25-40 ℃; the II-grade separation pressure is 7-8Mpa, and the temperature is 25-40 ℃;
in step B2, the filtration is performed with a 0.1-0.22um filter membrane.
5. Use of the camellia japonica thunb combined extract according to claim 1 in cosmetics.
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